CN101323173A - Composite material sheet and production method thereof - Google Patents
Composite material sheet and production method thereof Download PDFInfo
- Publication number
- CN101323173A CN101323173A CNA2007101379706A CN200710137970A CN101323173A CN 101323173 A CN101323173 A CN 101323173A CN A2007101379706 A CNA2007101379706 A CN A2007101379706A CN 200710137970 A CN200710137970 A CN 200710137970A CN 101323173 A CN101323173 A CN 101323173A
- Authority
- CN
- China
- Prior art keywords
- filler
- organic resin
- composite
- composite material
- material sheet
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000002131 composite material Substances 0.000 title claims abstract description 197
- 238000004519 manufacturing process Methods 0.000 title description 7
- 239000000945 filler Substances 0.000 claims abstract description 151
- 229920005989 resin Polymers 0.000 claims abstract description 146
- 239000011347 resin Substances 0.000 claims abstract description 146
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- 239000011159 matrix material Substances 0.000 claims abstract description 57
- 239000002245 particle Substances 0.000 claims description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 239000000463 material Substances 0.000 claims description 30
- 238000002360 preparation method Methods 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 25
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- 239000003960 organic solvent Substances 0.000 claims description 10
- 241000555268 Dendroides Species 0.000 claims description 8
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- 230000000052 comparative effect Effects 0.000 description 25
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- 229910002113 barium titanate Inorganic materials 0.000 description 10
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 9
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- 239000000843 powder Substances 0.000 description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
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- 229910052582 BN Inorganic materials 0.000 description 5
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 5
- 239000003990 capacitor Substances 0.000 description 5
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- 238000005259 measurement Methods 0.000 description 5
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- 229920000178 Acrylic resin Polymers 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 4
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- 239000004698 Polyethylene Substances 0.000 description 2
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- FRWYFWZENXDZMU-UHFFFAOYSA-N 2-iodoquinoline Chemical compound C1=CC=CC2=NC(I)=CC=C21 FRWYFWZENXDZMU-UHFFFAOYSA-N 0.000 description 1
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- 229910017083 AlN Inorganic materials 0.000 description 1
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910001021 Ferroalloy Inorganic materials 0.000 description 1
- 239000002879 Lewis base Substances 0.000 description 1
- 235000015511 Liquidambar orientalis Nutrition 0.000 description 1
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- 239000004952 Polyamide Substances 0.000 description 1
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- 239000004721 Polyphenylene oxide Substances 0.000 description 1
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- 239000004793 Polystyrene Substances 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 239000004870 Styrax Substances 0.000 description 1
- 244000028419 Styrax benzoin Species 0.000 description 1
- 235000000126 Styrax benzoin Nutrition 0.000 description 1
- INPODWZONOWTET-UHFFFAOYSA-N [Nb].[Mg].[Zn] Chemical compound [Nb].[Mg].[Zn] INPODWZONOWTET-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
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- 239000002585 base Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- LTPBRCUWZOMYOC-UHFFFAOYSA-N beryllium oxide Inorganic materials O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 description 1
- 239000011469 building brick Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
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- 238000006243 chemical reaction Methods 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- XLJMAIOERFSOGZ-UHFFFAOYSA-M cyanate Chemical compound [O-]C#N XLJMAIOERFSOGZ-UHFFFAOYSA-M 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
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- 238000001227 electron beam curing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
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- 229910052736 halogen Inorganic materials 0.000 description 1
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- MRNHPUHPBOKKQT-UHFFFAOYSA-N indium;tin;hydrate Chemical compound O.[In].[Sn] MRNHPUHPBOKKQT-UHFFFAOYSA-N 0.000 description 1
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- 150000002500 ions Chemical class 0.000 description 1
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- 239000011968 lewis acid catalyst Substances 0.000 description 1
- 150000007527 lewis bases Chemical class 0.000 description 1
- 239000004611 light stabiliser Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
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- 238000001000 micrograph Methods 0.000 description 1
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- 150000004767 nitrides Chemical class 0.000 description 1
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- 229920005644 polyethylene terephthalate glycol copolymer Polymers 0.000 description 1
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- 239000011116 polymethylpentene Substances 0.000 description 1
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- 230000001376 precipitating effect Effects 0.000 description 1
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- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 description 1
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- 239000000377 silicon dioxide Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
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- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
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- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 229920006337 unsaturated polyester resin Polymers 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/58—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising fillers only, e.g. particles, powder, beads, flakes, spheres
- B29C70/62—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising fillers only, e.g. particles, powder, beads, flakes, spheres the filler being oriented during moulding
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/88—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts characterised primarily by possessing specific properties, e.g. electrically conductive or locally reinforced
- B29C70/882—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts characterised primarily by possessing specific properties, e.g. electrically conductive or locally reinforced partly or totally electrically conductive, e.g. for EMI shielding
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/16—Non-insulated conductors or conductive bodies characterised by their form comprising conductive material in insulating or poorly conductive material, e.g. conductive rubber
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/20—Dielectrics using combinations of dielectrics from more than one of groups H01G4/02 - H01G4/06
- H01G4/206—Dielectrics using combinations of dielectrics from more than one of groups H01G4/02 - H01G4/06 inorganic and synthetic material
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/03—Use of materials for the substrate
- H05K1/0313—Organic insulating material
- H05K1/0353—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement
- H05K1/0373—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement containing additives, e.g. fillers
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/16—Printed circuits incorporating printed electric components, e.g. printed resistor, capacitor, inductor
- H05K1/162—Printed circuits incorporating printed electric components, e.g. printed resistor, capacitor, inductor incorporating printed capacitors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
- B29K2105/06—Condition, form or state of moulded material or of the material to be shaped containing reinforcements, fillers or inserts
- B29K2105/16—Fillers
- B29K2105/18—Fillers oriented
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2705/00—Use of metals, their alloys or their compounds, for preformed parts, e.g. for inserts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2709/00—Use of inorganic materials not provided for in groups B29K2703/00 - B29K2707/00, for preformed parts, e.g. for inserts
- B29K2709/02—Ceramics
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2995/00—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds
- B29K2995/0003—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds having particular electrical or magnetic properties, e.g. piezoelectric
- B29K2995/0006—Dielectric
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2995/00—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds
- B29K2995/0012—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds having particular thermal properties
- B29K2995/0013—Conductive
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2031/00—Other particular articles
- B29L2031/30—Vehicles, e.g. ships or aircraft, or body parts thereof
- B29L2031/3055—Cars
- B29L2031/3061—Number plates
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
- H05K2201/02—Fillers; Particles; Fibers; Reinforcement materials
- H05K2201/0203—Fillers and particles
- H05K2201/0206—Materials
- H05K2201/0209—Inorganic, non-metallic particles
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
- H05K2201/02—Fillers; Particles; Fibers; Reinforcement materials
- H05K2201/0203—Fillers and particles
- H05K2201/0242—Shape of an individual particle
- H05K2201/0251—Non-conductive microfibers
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2203/00—Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
- H05K2203/10—Using electric, magnetic and electromagnetic fields; Using laser light
- H05K2203/105—Using an electrical field; Special methods of applying an electric potential
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/249921—Web or sheet containing structurally defined element or component
- Y10T428/249994—Composite having a component wherein a constituent is liquid or is contained within preformed walls [e.g., impregnant-filled, previously void containing component, etc.]
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Abstract
The present invention provides a composite material sheet wherein a filler is oriented in a given direction in an organic resin matrix by an electric field. The composite material sheet of the present invention 10 contains filler 1 and organic resin 3, and is characterized in that the filler 1 is dendritically aggregated in the organic resin matrix and oriented in the thickness direction. As a result, properties such as dielectric property, conductivity, thermal conductivity and the like can be strikingly improved as compared to conventional composite materials obtained by simply dispersing a filler.
Description
Technical field
The application relates to a kind of composite material sheet and manufacture method thereof.More specifically, the application relate to a kind of dielectric properties etc. excellent, can be as such as the electronics of printed circuit board (PCB), capacitor, semiconductor sealing resin encapsulation etc. or the composite material sheet and the manufacture method thereof of electric component.
Background technology
Usually, the composite of one or more fillers dispersed in the organic resin matrix has been applied to multiple field.But, because the composite of current use prepares fillers dispersed simply by using ball mill etc. in the organic resin matrix, therefore after they are by long-term the placement, thereby the filler bigger than organic resin density can precipitatedly cause uneven density easily, and this uneven density is difficult to obtain uniform composite conversely.
In order to address the above problem, to attempt utilizing external field to make filler orientation, and fix this state of orientation according to the direction that provides in the organic resin matrix.Field as the outside, flow field, magnetic field, electric field, ultrasonic field etc. have been used, for example publication number is that JP-A-2001-185261 discloses a kind of anisotropic conductive sheet, the ferromagnetic particle of wherein conducting electricity is orientated on the sheet thickness direction, this is by being placed on composite between a pair of relative metal die magnetic pole, and apply magnetic field and locate conduction ferromagnet particle and solidify insulative polymer material and obtain, the ferromagnetic particle of wherein conducting electricity is dispersed in the insulation polymer material.
Yet when using the magnetic field of electromagnet rank intensity, the kind of available filler is restricted to the ferromagnetic material of iron, nickel and cobalt.Though use superconducting magnet to provide to allow the high-intensity magnetic field intensity of using the material beyond the ferromagnetic material, be used to develop the device costliness of cryogenic magnetic field, and the zone that the development of superconduct magnetic field occurs is limited in the problem of about 100mm etc.
On the other hand, when using electric field, also can advantageously use ferromagnetic material inorganic material in addition as the outfield.For example, JP-A-2004-193411 has proposed the method that a kind of preparation has the electric or electronic building brick of high-k, this assembly is in the same place by raw polymer is kneaded with the powder with high-k, add solvent and obtain having the paste that to control viscosity, obtain film and it is applied electric field thereby paste is applied over conductive substrates.
Yet JP-A-2004-193411 does not have report or even does not have to advise that the powder with high-k can be orientated in the direction that provide by film is applied electric field.In addition, according to discovering of the inventor, when to by epoxy resin being dissolved in the organic solvent (MEK) and adding and the composite that disperses barium titanate to obtain applies electric field, and during the heat cure above-mentioned material, according to the described method of JP-A-2004-193411, barium titanate is orientation not, therefore do not obtain practical composite, in addition, when electric field is applied to coated film, can obtain similar result, thereby wherein this coated film obtains by the above-mentioned paste removal of drying organic solvent.As mentioned above, according to present circumstances, there is not recognized techniques to be used at the organic resin matrix filler being orientated in given direction by electric field.
Summary of the invention
[technical problem to be solved by this invention]
Consider that said circumstances finished the present invention, it is a kind of wherein by electric field filler composite materials film and manufacture method thereof in given direction orientation in the organic resin matrix that purpose is to provide.
[method of dealing with problems]
The inventor has carried out deep research in order to address the above problem, and find as mentioned above, can not obtain by electric field composite materials at given direction oriented padding in the organic resin matrix, this is that composite can be extruded on the exterior circumferential of electrode simultaneously because the organic solvent in paste can evaporate when applying electric field and heat cure.Based on above-mentioned discovery, discover that further the composite that filler is orientated according to given direction can be by preparation wherein not with an organic solvent in the organic resin matrix, the composite of fillers dispersed in the organic resin matrix do not applied alternating voltage to it obtain, thereby finish the present invention.
Thereby, the invention provides as follows:
(1) a kind of composite material sheet that comprises filler and organic resin matrix, wherein filler is converged into dendroid and is orientated on the thickness direction of organic resin matrix.
(2) composite material sheet of above-mentioned (1), wherein the degree of orientation of filler is greater than 1.05.
(3) composite material sheet of above-mentioned (1) or (2), wherein the dielectric constant of filler is greater than the dielectric constant of organic resin.
(4) any one composite material sheet in above-mentioned (1) to (3), wherein filler is at least a in inorganic particulate and the inorfil.
(5) any one composite material sheet in above-mentioned (1) to (4), wherein the content with respect to the organic resin filler is 5-60vol%.
(6) a kind of dielectric sheet material, it comprises any one composite material sheet in above-mentioned (1) to (5) and at least a as in the dielectric inorganic particle of filler and the dielectric inorganic fiber.
(7) a kind of heat exchange sheet material, it comprises any one composite material sheet in above-mentioned (1) to (5) and at least a as in the heat of filler conduction inorganic particulate and the heat conduction inorfil.
(8) a kind of anisotropic conductive sheet material, it comprises any one composite material sheet in above-mentioned (1) to (5) and at least a as in the conduction inorganic particulate of filler and the conduction inorfil.
(9) a kind of method for preparing composite material sheet, wherein filler is orientated on the assigned direction of organic resin matrix, this method comprises: the step of kneading, this step comprises that with an organic solvent do not knead organic resin and filler obtain composite, this composite has the water content that is no more than 0.30wt%, and wherein filler is dispersed in the organic resin matrix; Electric field treatment step, this step comprise on the composite paint electrode, perhaps composite injected or be placed between the electrode, and apply alternating voltage, thereby filler is orientated on given direction; And fixing step, be fixed in the organic resin matrix with filler orientation.
(10) a kind of method for preparing composite material sheet, wherein filler is orientated on the assigned direction of organic resin matrix, this method comprises: the step of kneading, this step comprises that with an organic solvent do not knead organic resin and filler obtain composite, this composite has the water content that is no more than 0.30wt%, and wherein filler is dispersed in the organic resin matrix; Electric field treatment step, this step comprise with resin film and are coated with composite, apply alternating voltage, thereby filler is orientated on given direction; And fixing step, be fixed in the organic resin matrix with filler orientation.
(11) preparation method of above-mentioned (9) or (10), wherein in the electric field treatment step, filler is orientated on thickness direction as the dendroid aggregation.
(12) any one preparation method in above-mentioned (9) to (11), wherein filler has the dielectric constant higher than organic resin.
(13) any one preparation method in above-mentioned (9) to (12), wherein filler is at least a in inorganic particulate and the inorfil.
(14) any one preparation method in above-mentioned (9) to (13), wherein, in the step of kneading, use filler and organic resin to prepare composite, make the ratio (A/B) of dielectric constant (B) of the dielectric constant (A) of filler and organic resin be not less than 10, the particle mean size of this filler is not less than 1 μ m, and in the electric field treatment step, the alternating voltage that electric-field intensity is not less than 0.1kV/mm is applied on the composite.
(15) any one preparation method in above-mentioned (9) to (13), wherein, in the step of kneading, use filler and organic resin to prepare composite, make the ratio (A/B) of dielectric constant (B) of the dielectric constant (A) of filler and organic resin less than 10, the particle mean size of this filler is not less than 1 μ m, and in the electric field treatment step, the alternating voltage that electric-field intensity is not less than 1kV/mm is applied on the composite.
(16) any one preparation method in above-mentioned (9) to (13), wherein, in the step of kneading, use filler and organic resin to prepare composite, make the ratio (A/B) of dielectric constant (B) of the dielectric constant (A) of filler and organic resin be not less than 10, the particle mean size of this filler is less than 1 μ m, and in the electric field treatment step, the alternating voltage that electric-field intensity is not less than 1kV/mm is applied on the composite.
(17) any one preparation method in above-mentioned (9) to (13), wherein, in the step of kneading, use filler and organic resin to prepare composite, make the ratio (A/B) of dielectric constant (B) of the dielectric constant (A) of filler and organic resin be set to less than 10, the particle mean size of this filler is less than 1 μ m, and in the electric field treatment step, the alternating voltage that electric-field intensity is not less than 10kV/mm is applied on the composite.
[invention effect of the present invention]
According to the present invention, a kind of composite material sheet is provided, wherein filler is converged into dendroid and is orientated on thickness direction in the organic resin matrix.The result is, because with compare by disperseing filler to obtain conventional composite simply, composite material sheet of the present invention can improve significantly such as character such as dielectric properties, electric conductivity, heat conductivities, therefore it can be applied to the multiple field that comprises electronics and electric component, for example printed circuit board (PCB), capacitor, semiconductor sealing resin encapsulation etc.In addition, preparation in accordance with the present invention, because electric field is used as external field, multiple material can be used as filler.In addition owing to do not need expensive process units especially, therefore can be expediently and be provided at the composite material sheet of aspect excellences such as dielectric properties, electric conductivity, heat conductivity with low cost.
Description of drawings
Fig. 1 shows the figure of an embodiment of composite material sheet of the present invention.
Fig. 2 shows the figure of another embodiment of composite material sheet of the present invention.
Fig. 3 is the schematic diagram that an embodiment of the electric field treatment device that is used to prepare composite material sheet of the present invention is shown.
Fig. 4 is the schematic diagram that another embodiment of the electric field treatment device that is used to prepare composite material sheet of the present invention is shown.
Fig. 5 illustrates the heating curves of the composite material sheet of preparation embodiment and Comparative Examples.
Fig. 6 shows the filer content of composite material sheet and the relation between the dielectric constant.
Fig. 7 is the optics micrograph of the composite material sheet of acquisition among embodiment 2 and the embodiment 3 along Ia-Ia direction cross section.
Fig. 8 obtains the SEM photo of composite material sheet along Ia-Ia direction cross section among the embodiment 4.
Fig. 9 is the SEM photo of the composite material sheet of acquisition among the embodiment 4 along Ib-Ib direction cross section.
Figure 10 is the SEM photo of the composite material sheet of acquisition in the Comparative Examples 4 along Ia-Ia direction cross section.
Figure 11 is the SEM photo of the composite material sheet of acquisition in the Comparative Examples 4 along Ib-Ib direction cross section.
[symbol description]
1: filler, 3: organic resin, 10: composite material sheet
The specific embodiment
[implementing optimal mode of the present invention]
Below by the invention has been described in detail with reference to preferred embodiment.In description of drawings, identical element adopts identical mark, and therefore the explanation that repeats is omitted.Statement for convenience, the dimension scale of accompanying drawing is not necessarily consistent with the statement of specification.
(composite material sheet)
Composite material sheet of the present invention is characterised in that filler is converged on dendroid and the thickness direction in the organic resin matrix and is orientated.
Fig. 1 shows an embodiment of composite material sheet.
Fig. 1 (a) is the perspective view of composite material sheet 10, and Fig. 1 (b) is the schematic cross-section of composite material sheet 10 along the Ia-Ia line.In the composite material sheet 10 of the present embodiment, filler 1 forms band shape or chain-cluster body, and its thickness direction (z direction of principal axis) in the organic resin matrix is gone up and extended, and the aggregation of filler 1 diverges from here as trunk further.The end portion of aggregation is exposed at least one surface of sheet material.That is, the aggregation of filler 1 forms dendroid on the whole, and goes up orientation at thickness direction (z direction of principal axis).In addition, the aggregation of many fillers 1 is present in the organic resin matrix, and adjacent aggregation is connected to each other together and forms a for example network structure (for example honeycomb, ladder) each other.
Therefore, in the composite material sheet of this embodiment, because the filler aggregation is not only arranged on thickness direction, and diverge, therefore compare with the conventional composite materials that the column filler only is orientated on thickness direction, conductive path increases, and the conduction efficiency of electricity and heat improves.The result is that the dielectric properties of composite material sheet, electric conductivity and heat conductivity are significantly improved.Therefore, the composite material sheet of this embodiment is preferably as the electric or electronic unit (for example dielectric sheet material) that needs high dielectric property, for example printed circuit board (PCB), capacitor etc.; Electric or the electronic unit (for example heat exchange sheet material) that needs high-termal conductivity, for example printed circuit board (PCB), semiconductor sealing resin encapsulation etc.; Be used for multiple spot simultaneously electricity and for example IC etc. and printed circuit board (PCB) etc. of the electric or electronic unit of linkage function element (for example anisotropic conductive sheet material) fine.
Fig. 2 is the schematic sectional view that illustrates in another embodiment of composite material sheet.
In the composite material sheet 20 shown in Fig. 2 (a), because constituting the aggregation of trunk is orientated on the direction that tilts with respect to thickness direction (z direction of principal axis), but other structure is identical with composite material sheet 10, therefore, the differently-oriented directivity of composite material sheet 20 is different from composite material sheet 10, and wherein the differently-oriented directivity of composite material sheet 10 is at the z direction of principal axis.Therefore, as composite material sheet 10, sheet material 20 can have superior dielectric properties, good electric conductivity and good heat conductivity and excellent making as dielectric piece material, heat exchange sheet material and anisotropic conductive sheet material etc.
As mentioned above, the filler that constitutes composite material sheet of the present invention is orientated on thickness direction, and degree of orientation characteristic ground is greater than 1.05.Here, degree of orientation is meant the value of calculating by the following method.Particularly, obtain the SEM photo by using SEM (SEM, model S-4700, Hitachi, Ltd. manufacturing), the SEM image in sheet material cross section is trimmed (512 * 512 pixels, 25.4 μ m * 25.4 μ m).Then, use image processing software (ImageJ, United States National Institutes of Health makes) image is made two-dimension fourier transform, obtain the section (width of 100 pixels) of about 20% width of average entire image from the center.Make image and Gaussian function coupling (matching range is 30%, 150 a whole pixel) then, and measure in the adaptation function at half-breadth C on the longitudinal direction (direction that is parallel to electric field) and the half-breadth D on horizontal direction (perpendicular to the direction of electric field).The ratio that calculates D/C is as degree of orientation.For the curve coupling, used image to generate software (IGOR, WaveMetrics makes).
Degree of orientation by using the filler that said method calculates preferably is not less than 1.1 generally greater than 1.05, more preferably is not less than 1.2, further preferably is not less than 1.3.By this degree of orientation is set, electronics and electric device for example in printed circuit board (PCB), capacitor, the semiconductor sealing resin encapsulation etc. required various performances for example dielectric properties, electric conductivity, heat-conductive characteristic get can arrive significantly and improve.
In addition, the water content of composite material sheet preferably is no more than 0.30wt%, more preferably no more than 0.20wt%, further preferably be no more than 0.10wt%, especially preferably be no more than 0.05wt%, by this water content is set, for example performances such as dielectric properties, electric conductivity, heat conductivity can further improve.In this manual, water content is measured according to JIS K0068.
The thickness of composite material sheet is suitably determined according to applied object, is generally 10-500 μ m, is preferably 50-200 μ m.
The structural constituent of composite material sheet of the present invention illustrates in following content.
Organic resin plays matrix in composite, and gives composite such as processing characteristics and flexible performance.As organic resin, preferably use the organic resin that when applying electric field, allows filler in the organic resin matrix, to move with flowability.That is, when the content of filler hangs down, even when organic resin has higher relatively viscosity, can obtain needed state of orientation by applying electric field Moveable packings in the organic resin matrix.When the content of filler is high, be not easy to obtain needed state of orientation, unless the viscosity of organic resin is set to lower level.Therefore, the content of filler and the viscosity of organic resin such as required strategic point are adjusted, so that filler can move in the organic resin matrix at an easy rate when applying electric field.
As organic resin, preferably for example thermoplastic resin, thermosetting resin, light-cured resin, electron beam (EB) cured resin etc.In the situation of thermosetting resin and light-cured resin, the preferred material that uses liquid state or have flowability in room temperature.Though the viscosity of organic resin is according to the performance (for example content, granularity, shape, surface roughness (skin friction resistance)) of filler, the changes such as (for example electric field frequency, electric-field intensity, application time, temperature) of the applying condition of electric field, but for example viscosity is generally 10-2000mPaS in the time of 25 ℃, is preferably 10-200mPaS.Here, by using JIS 7117-1B type viscosimeter to measure viscosity.
As thermoplastic resin, can use polyimide resin, polyamide, polyamide-imide resin, polyphenylene oxide, PPSU etc., preferably use polyimide resin.
In addition,, can use epoxy resin, phenolic resin, organic siliconresin, unsaturated polyester resin, BMI (bismaleid) resin, cyanate resin etc., preferably use epoxy resin as thermosetting resin.As epoxy resin, the preferred use by mixing as for example aliphatic poly epihydric alcohol base of the aliphatic epoxy resin ether of basic resin etc., and the liquid-state epoxy resin of curing agent (for example acid anhydrides) and curing accelerator (for example tertiary amine, lewis acid catalyst based) acquisition.The mixing ratio of each component can suitably be determined according to purpose.
As light-cured resin, can use ultraviolet ray (UV) cured resin etc.As light or electron beam curing resin, the preferred liquid cured resin of for example making that uses by the mixture of oligomer such as epoxy acrylate, urethane acrylate etc., reaction dilution and Photoepolymerizationinitiater initiater (for example styrax, acetophenone etc.).The mixing ratio of each component is suitably determined according to purpose.
Filler disperses, and gives for example various performances of dielectric properties, electric conductivity and heat conductivity of composite thus.Filler does not have special restriction, as long as it has the dielectric constant that is higher than matrix resin, for example can use pottery, metal, alloy and organic resin.The shape of filler also has no particular limits, and for example can use sphere, ellipse, aciculiform, plate shape, fiber etc., preferably uses sphere and fiber.Above-mentioned shape can be used separately, also can two or more shape be used in combination simultaneously.
As filler, generally use inorganic particulate, inorfil, organic resin particle etc., preferably use inorganic particulate and inorfil.As inorganic particulate, for example can use metal or nonmetallic carbide, nitride, oxide etc.Particularly, can use inorganic powder, for example carborundum, silicon nitride, boron nitride, aluminium oxide, barium titanate, tin oxide, tin-antiomony oxide, titanium oxide/tin-antiomony oxide, tin indium oxide etc.As inorfil, for example can use ceramic fibre such as barium titanate, aluminium oxide, silica, carbon etc., metallic fiber such as iron, copper etc., the ceramic fibre of preferred use such as barium titanate etc.As the organic resin particle, for example can use vistanex powder, acrylic resin, polystyrene resin, fluororesin, organic siliconresin and their mixture such as polyethylene, polypropylene, polymethylpentene etc.For example, acrylic resin particle (as crosslinked acrylic resin particle, non-crosslinked acrylic resin particle) can MX series, MR series and MP series (as described in series all be SOKEN CHEMICAL ﹠amp; ENGINEERING CO., the trade name of LTD.) be purchased, and styrene resin beads (as the crosslinked polystyrene particle) can SX series and SGP series be purchased.
For example, can use the particle (particle with core/shell double-layer structure) with double-layer structure, wherein metallic is as core and its outer surface is coated with inorganic oxide.Can use the particle with double-layer structure particularly, wherein copper particle is as core and its outer surface is coated with barium titanate.And having difform filler can be used in combination.For example, when the inorfil that will have nano-sized diameters such as CNT and inorganic spherical particle are used in combination, can obtain bonding to form the filler aggregation of chain.Fig. 2 (b) is the schematic cross-section of composite material sheet 30, and wherein filler 1 is the combination of inorfil 1a and inorganic particulate 1b.By this structure, adopt less filer content can represent excellent dielectric properties, electric conductivity and heat conductivity.
When inorganic particulate or organic resin particle during as filler, the preferred particle that has about uniform grain sizes and in size distribution, do not disperse that uses.The particle mean size of filler is generally 0.5nm-100 μ m, is preferably 10nm-20 μ m, more preferably 100nm-10 μ m.When granularity during, because the Brownian movement of filler makes the response trend to electric field reduce less than 0.5nm.On the other hand, when granularity during greater than 100 μ m, because the gravity effect makes filler trend towards precipitating thereby be not easy to obtain required state of orientation.
In specification of the present invention, particle mean size is represented by using laser diffraction granularity apparatus for measuring distribution (Ltd. makes for LA-920 type, Horiba) to measure the particle mean size (D50) that employed filler obtains.When particle mean size is 0.1 μ m or when lower, expression is by measuring the particle mean size (D50) that obtains with dynamic light scattering particle size distributional analysis instrument (Inc. makes for N5 type, Beckman Coulter).
In addition, as inorfil, use fibre diameter to be generally 1nm-10 μ m, be preferably 10nm-1 μ m, fibre length is generally 10nm-100 μ m, is preferably 0.1 μ m-100 μ m and their aspect ratio and generally is not less than 10, is preferably and is not less than 100 inorfil.
With respect to the organic resin that constitutes matrix, the content of filler is preferably 5-60vol%, and more preferably 10-40vol% also is preferably 20-30vol%.When content during, when applying electric field, because filler by step by step rather than be orientated continuously, therefore can not easily obtain needed state of orientation less than 5vol%.On the other hand,, can not easily prepare composite, and the processing characteristics of sheet material and flexible being tending towards reduce when content during greater than 60vol%.
In addition, owing to contain the filler with desired properties, therefore composite material sheet of the present invention can provide the Electrical and Electronic product that is fit to purpose.
For example, dielectric inorganic particle and dielectric inorganic fiber at least a as filler, and being orientated on its direction that provides in the organic resin matrix for example can obtain having the dielectric sheet material that is not less than 10 high-k.So long as when having the inorganic material of dielectric properties and just not limiting especially, for example can use barium titanate, metatitanic acid zinc-magnesium niobium, strontium titanates etc., preferably use barium titanate when dielectric inorganic particle and dielectric inorganic fiber.As the dielectric sheet material, for example can use condenser sheet material with high-k or capacitor sheet material with high-k.In specification of the present invention, according to JIS K 6911 Measuring Dielectric Constant.
And, use at least a in heat conduction inorganic particulate and the heat conduction inorfil, the heat exchange sheet material that for example can obtain to have the high heat conductance that is not less than 2W/mK as filler.When heat conduction inorganic particulate and heat conduction inorfil so long as when having the inorganic material of thermal conductivity and just not limiting especially, for example can use beryllium oxide, aluminium nitride, boron nitride, carborundum, aluminium oxide, magnesia, titanium oxide etc., preferably use boron nitride.In specification of the present invention, measure pyroconductivity according to ASTME1530.
In addition, use at least a in conduction inorganic particulate and the conduction inorfil, for example can obtain to have by being not more than 1 * 10 as filler
4The anisotropic conductive sheet material of the excellent electric conductivity that the specific insulation of Ω cm is represented.Conduction inorganic particulate and conduction inorfil preferably use gold-plated nickel particles so long as the inorganic material with conductivity with regard to restriction especially, for example can be used gold-plated nickel particles, silver particles, gold particle, gold plated polymer particle etc.In specification of the present invention, according to JIS K 7194 measurement volumes resistivity.
More than composite material sheet of the present invention done detailed explanation by the reference implementation scheme, but can not be interpreted as that it has done qualification to the present invention.Can do multiple modification and change to the present invention without departing from the scope of the invention.According to application target, composite material sheet can comprise additive, for example antioxidant, thermostabiliser, light stabilizer, ultra-violet absorber, lubricant, antifoggant, anticaking agent, colouring agent, fire retardant, antistatic additive, electric conductivity imparting agent etc. can suitably be determined their ratio.In addition, composite material sheet can be processed according to application purpose.Under the situation of dielectric sheet material, for example can remove battery lead plate and form new electrode by Wet-type etching.
(preparation method of composite material sheet)
The preparation method of composite material sheet of the present invention is characterised in that it comprises: the step of kneading, electric field treatment step and fixing step.Each step all elaborates below.
At first, preparation organic resin and filler.
Orientation is subjected to the influence of conductive component content in the composite on the direction whether filler provides in the organic resin matrix.Therefore, wish that conductive component content is as far as possible little in the composite.As conductive component, can mention water and ion component, for example halogen ion, metal ion etc., and the influence of water is big especially.
In this case, the water content among the present invention in the composite is set to and is not more than 0.30wt%, preferably is not more than 0.20wt%, more preferably no more than 0.10wt%, further preferably is not more than 0.05wt%.In order to obtain containing the composite of above-mentioned water content, preferred following material is as organic resin and filler.The water content of this composite be illustrated in to apply electric field at once before, the water content of the composite of measuring according to JIS K0068 above-mentioned.
As organic resin, use its water content preferably to be not more than 0.1wt%, more preferably no more than the organic resin of 0.05wt%.In order to obtain above-mentioned water content, ideally organic resin is positioned over dry or preservation in the drier.In this case, the inside of wishing drier is set to argon atmospher.
As filler, use its water content preferably to be not more than the filler of 0.1wt%, more preferably water content is not more than 0.05wt%.In order to obtain above-mentioned water content, filler only needs heat drying, and the condition of heat drying is 150-350 ℃/1-10hr for example, is preferably 200-300 ℃/2-3hr.When the content of water has surpassed above-mentioned scope, apply during the electric field filler can be in the organic resin matrix strenuous exercise, therefore be difficult to provide the state of orientation that needs.Measure water content according to JIS K 0068 above-mentioned.
Then, the step of kneading.In the step of kneading, with an organic solvent organic resin is not kneaded with filler and be in the same place, thereby obtain the composite that water content is not more than 0.30wt%, wherein fillers dispersed is in the organic resin matrix.In the present invention since during the preparation composite not with an organic solvent, at room temperature be that liquid organic resin or heating can become flowable organic resin as organic resin so use.With respect to organic resin, the content of employed filler is preferably 5-60vol%, and more preferably 10-40vol% further is preferably 20-30vol%.
The method of fillers dispersed in the organic resin matrix is not particularly limited, can uses known dispersal device for example ball mill, dispersing mixer, kneading machine etc. according to the viscosity of organic resin.Before applying electric field, when filler forms a solid aggregation, in the electric field treatment step of mentioning below, the orientation difficulty that will become on assigned direction.Therefore, need carry out sufficient dispersion treatment.
Then, carry out the electric field treatment step.In the electric field treatment step, be orientated on the direction of regulation in order to make filler, the composite that obtains in the step of kneading is applied an alternating voltage.
Fig. 3 is the schematic diagram that an embodiment of the electric field treatment device that is used to prepare composite material sheet of the present invention is shown.In electric field treatment device 100, a pair of electrode of opposite 103 is arranged in the chamber 101, and composite 105 is placed between the electrode 103.Electrode 103 for example is a conductivity substrate, and wherein Copper Foil attaches on the SUS carrier by the conduction double-sided belt.Electrode 103 is connected to an amplifying device 107 and the voltage generator 109 that can apply electric field to composite 105 at desired conditions.
When matrix resin is during at normal temperatures for liquid thermosetting resin or light-cured resin, for the flaky composite material of preparation facilities between electrode, for example composite is injected between the electrode or and is coated on the electrode to obtain coated film with composite.When matrix resin is during at room temperature for solid-state thermoplastic resin, for example composite is kneaded in extruder, and composite is processed to sheet material by extrusion molding etc., and is placed between the electrode.The thickness of flaky composite material is generally 10-500 μ m, is preferably 50-200 μ m.
Fig. 4 is the schematic diagram that another embodiment of electric field treatment device is shown.In electric field treatment device 120, roller shape electrode 113 is arranged in the chamber 101, and the feeding parts 115 that are used for adding composite 105 also are arranged in the chamber 101, this on the one hand its structure be different from electric field treatment device 100.Electrode 113 is the conductive drum for being made by conducting metal (for example copper alloy, ferroalloy) for example.The surface coverage resin film 117 of composite 105.
When matrix resin is during at room temperature for liquid thermosetting resin or light-cured resin, in order to prepare the composite that resin film is arranged in its surface applied, thereby for example composite is coated on resin film and forms the coating film, then resin film is positioned on the coating film.When matrix resin is during at room temperature for solid-state thermoplastic resin, for example with composite and resin film by co-extrusion laminating to form flaky composite material.The thickness of composite as mentioned above.As resin film, preferably use polyolefin film (for example polyethylene film, polypropylene film), polyester film (for example PETG film) etc., its thickness is generally 5-50 μ m, is preferably 10-25 μ m.
Direction orientation for filler is provided in the organic resin matrix applies electric field to the flaky composite material that obtains.When necessary, during applying electric field, may need heating.When applying electric field, thereby filler is arranged in aggregation and forms trunk branch applying on the direction of electric field.In addition, be formed on the direction that applies electric field from branch that trunk extends out.The result is that the end of branch or trunk contacts with at least one electrode.Use the electric field treatment device shown in Fig. 3 and Fig. 4 (a), filler can be orientated as shown in Figure 1.In addition, by the downstream of an electrode in the mobile chamber to another electrode, shown in Fig. 4 (b), filler also may be orientated as shown in Fig. 2 (a).Use the electric field treatment device shown in Fig. 4 (a) and Fig. 4 (b), surface coverage has the composite of resin film can constantly carry out electric field treatment.The result is that the output of composite material sheet is improved significantly.
In the present invention, under following treatment conditions, adopt alternating voltage as electric field.And the inventor finds that when applying DC voltage filler can move tempestuously, has stoped the orientation of filler in the organic resin matrix.
Electric-field intensity is generally 0.1-50kV/mm, is preferably 1-25kV/mm, 3-20kV/mm more preferably, when its during less than 0.1kV/mm, the Brownian movement of filler becomes and occupies advantage, thereby can not easily obtain the state of orientation that needs.When its during greater than 50kV/mm, composite trends towards occurring dielectric breakdown.
Frequency is generally 0.1-1MHz, is preferably 0.1-100kHz, and more preferably 0.1-50kHz further is preferably 0.1-20kHz.When frequency has exceeded above-mentioned scope, can not easily obtain needed dispersity.
Though for the various matrix resin processing time difference of using, the general processing time is 0.01-2hr, is preferably 0.01-1hr, more preferably 0.01-0.1hr.When its during less than 0.01hr, it is not enough that the orientation of filler sometimes becomes, when its during greater than 2hr, composite trends towards occurring dielectric breakdown.
Consider the dielectric constant etc. of particle mean size, filler and the organic resin of filler, particularly preferably in carrying out electric field treatment under the condition shown in the table 1.
Table 1
Then, carry out fixing step.In fixing step, the filler aggregation that is orientated according to the direction that provides in the electric field treatment step is fixed in the organic resin matrix when keeping state of orientation.In the present invention, matrix resin can be selected according to application target.Matrix resin comprises instantaneous solidification, thereby easily the filler that will be orientated is fixed on the light-cured resin in the organic resin matrix, with up to solidifying or solidifying the thermoplastic resin and the thermosetting resin that filler could be fixed to according to state of orientation in the organic resin matrix, therefore need apply electric field incessantly.Therefore, in fixing step, can apply electric field incessantly.
When matrix resin during for thermosetting resin fixedly the method for filler for example be to comprise the method that is heating and curing.Though when condition of cure was suitably determined according to employed organic resin, solidification temperature was generally 100-200 ℃, be preferably 120-180 ℃ and be generally 1-10hr hardening time, be preferably 2-5hr.
When matrix resin is light-cured resin, for example can adopt the method for solidifying by irradiations such as ultraviolet rays.In this case, illumination penetrate can with apply electric field and carry out simultaneously, the substrate of photopermeability excellence (as ITO) can be used as electrode.Though illuminate condition can determine that rightly exposure intensity generally is not less than 200mW/cm according to employed organic resin
2, irradiation time is generally 1-10min, is preferably 3-5min.Need select exposure intensity and irradiation time to obtain to be not less than 2500mJ/cm rightly
2Illuminate condition.
In addition, when matrix resin is thermoplastic resin, for example can use the method that comprises cooled and solidified.
Preparation in accordance with the present invention, because electric field is used as the outfield, so filler can be orientated on a required direction in the organic resin matrix, and can not be subjected to the influence of employed carrier performance.In addition, preparation method of the present invention does not need special and expensive preparation facilities.Therefore, can be expediently and prepare needed composite material sheet at low cost.
The present invention has carried out more detailed explanation by specific embodiment in following content, but following content can not be interpreted as the present invention has been done qualification.
[embodiment]
(embodiment 1-5)
Prepare non-solvent epoxy resin by adding every kind of component described in the following table 2.The dielectric constant of the non-solvent epoxy resin that obtains is 3.3.
Table 2
| The whole seller | Model | Classification | Add quantity | |
| Main agents | Tohto kasei Co.，Ltd | ZX-1658 | |
100 weight portions |
| Curing agent | Japan Epo×yResin Co.，Ltd. | YH306 | Acid anhydrides | 160 weight portions |
| Curing accelerator | PTI Japan Ltd. | K-61B | Tertiary amine, lewis |
3 weight portions |
In the every part of non-solvent epoxy resin that is obtained, add barium titanate (BaTiO
3) powder (5,10,20 or 30vol%, BT-03, Sakai Chemical Industry Co., Ltd., make, particle mean size is 0.3 μ m, purity is not less than 99.9%, dielectric constant is approximately 3300), composite prepares by using planetary ball mill (model Planet-M, Gokin Planetaring makes) to carry out dispersion treatment.
The container and the ball that are used for dispersion treatment are prepared from by zirconia, are used in combination to have 1,2,4 or the ball of 8mm diameter.Treatment conditions are the 600rpm rotating speed, the 1500rpm rotating speed, and the processing time be 10 minutes.The water content of every part of composite is 0.03wt%.
Dynamic then viscoelastic device (MR-300V, Rheology Co., Ltd. make) be modified to provide the electric field treatment device, a upper electrode (1oz Copper Foil) and a lower electrode (3oz Copper Foil) are installed on it, each Copper Foil connects on the SUS carrier by a conduction double-sided belt.Then, composite is injected between two electrodes, and the quantity of breach is adjusted to the thickness of 50-100 μ m.Then when beginning to apply electric field, composite heats under the condition of as shown in Figure 5 heating curves.The electric field treatment condition is as shown in table 3.
After the cooling, from the electric field treatment device, take out the SUS carrier, be immersed in liquid nitrogen repeatedly and be exposed in the air.Conduction double-sided belt on the SUS carrier separates with Copper Foil makes composite material sheet have Copper Foil.The water content of every part of composite material sheet is 0.03wt%.
Table 3
(embodiment 6)
In the non-solvent epoxy resin that obtains by every part of component described in the interpolation table 2, add boron nitride powder (20vol%, model UHP-1, the hexagon boron nitride, Showa Denko K.K. makes, particle mean size 9.3 μ m, dielectric constant is approximately 4.5), and composite with embodiment 1 in the same mode obtain.The water content of composite is 0.03wt%.
Then, in the mode identical with embodiment 1, composite heats under the condition of as shown in Figure 5 heating curves, is 0.1kHz in frequency, and electric-field intensity is to apply alternating voltage under the 3kV/mm, thereby obtains the composite material sheet that thickness is 100 μ m.The water content of composite material sheet is 0.03wt%.
(embodiment 7)
In the non-solvent epoxy resin that obtains by every part of component described in the interpolation table 2, add gold-plated nickel particles (10vol%, FUKUDA MTEAL FOIL ﹠amp; POWDER CO., LTD. make, and particle mean size is 7.4 μ m, and gold plating thickness is 0.1-0.15 μ m), composite with embodiment 1 in identical mode obtain.The water content of composite is 0.03wt%.
Then, with embodiment 1 in identical mode, composite heats under the condition of as shown in Figure 5 heating curves, is 10kHz in frequency, electric-field intensity is to apply alternating voltage under the 16kV/mm, thereby obtains the composite material sheet that thickness is 100 μ m.The water content of composite material sheet is 0.03wt%.
(Comparative Examples 1)
Except not in non-solvent epoxy resin, not adding the barium titanate powder, obtained composite material sheet in the mode identical with embodiment 1.BaTiO in the composite material sheet
3The content of powder is as shown in table 4.
(Comparative Examples 2-5)
Except not carrying out the electric field treatment, obtained composite material sheet in the mode identical with embodiment 1-3 and embodiment 5.BaTiO in the composite material sheet
3The content of powder is as shown in table 4.
Table 4
| BaTiO 3Content | |
| Comparative Examples 1 | 0vol％ |
| Comparative Examples 2 | 5vol％ |
| Comparative Examples 3 | 10vol％ |
| Comparative Examples 4 | 20vol％ |
| Comparative Examples 5 | 30vol％ |
(Comparative Examples 6)
Except not carrying out the electric field treatment, obtained composite material sheet in the mode identical with embodiment 6.
(Comparative Examples 7)
Except not carrying out the electric field treatment, obtained composite material sheet in the mode identical with embodiment 7.
(Comparative Examples 8)
Have same composition and the composite of water content except using with embodiment 1, obtained composite material sheet in the mode identical with embodiment 1 as 0.36wt%.
(Comparative Examples 9)
Have same composition and the composite of water content except using with embodiment 2, obtained composite material sheet in the mode identical with embodiment 2 as 0.36wt%.
(Comparative Examples 10)
Have same composition and the composite of water content except using with embodiment 4, obtained composite material sheet in the mode identical with embodiment 4 as 0.36wt%.
(Comparative Examples 11)
Have same composition and the composite of water content except using with embodiment 5, obtained composite material sheet in the mode identical with embodiment 5 as 0.36wt%.
(assessment detects)
(1) dielectric properties
Remove the 1oz Copper Foil of upper electrode from the composite material sheet with Copper Foil that obtains among embodiment 1-5 and Comparative Examples 1-5 and 8-11, gold evaporation is to form the film main electrode on the surface of removing Copper Foil then, and sample is assessed in preparation thus.The electrode that uses impedance/phase gain analyzer (model HP4194A, Yokogawa-Hewlett-Packard makes) and be exclusively used in dielectric properties measuring instrument (model HP16451B), Measuring Dielectric Constant and dielectric tangent under the condition of 1kHz.Measurement result is shown in the table 5.The filer content of composite material sheet and the pass between the dielectric constant tie up to shown in the table 6.
(2) degree of orientation
Use SEM (SEM, model S-4700, Hitachi, Ltd. makes) obtain the SEM photo of the composite material sheet that in embodiment 1-7 and Comparative Examples 2-5 and 8-11, obtains, SEM image on the sheet material cross section is trimmed (512 * 512 pixels, 25.4 μ m * 25.4 μ m).Use image processing software (ImageJ, United States National Institutes of Health), image is made two-dimension fourier transform, obtain the section of about 20% width of average entire image.Make image and Gaussian function coupling (matching range is 30%, 150 a whole pixel) then, and measure in the adaptation function at half-breadth C on the longitudinal direction (direction that is parallel to electric field) and the half-breadth D on horizontal direction (perpendicular to the direction of electric field).Calculate the ratio of D/C as degree of orientation.Measurement result is shown in the table 5.For the curve coupling, used image to generate software (IGOR, Wave Metrics makes).
Fig. 7 (a) is the SEM figure of the composite material sheet of acquisition among the embodiment 2 along Ia-Ia direction cross section, and Fig. 7 (b) is the optical microscope photograph of the composite material sheet of acquisition among the embodiment 3 along Ia-Ia direction cross section.Fig. 8 (a) shows among the embodiment 4 in the composite material sheet that obtains the SEM figure along Ia-Ia direction cross section, and Fig. 8 (b) is the enlarged drawing of kernel of section.In addition, Fig. 9 (a) be the composite material sheet that obtains among the embodiment 4 along the SEM and the Fig. 9 (b) in Ib-Ib direction cross section is the enlarged drawing of kernel of section.Figure 10 (a) is the SEM figure of the composite material sheet of acquisition in the Comparative Examples 4 along Ia-Ia direction cross section, and Figure 10 (b) is the enlarged drawing of kernel of section.Figure 11 (a) is the composite material sheet that obtains in the Comparative Examples section S EM figure along the Ib-Ib direction, and Figure 11 (b) is the enlarged drawing of kernel of section.
Determine the optical microscope photograph from composite material sheet along Ia-Ia direction (thickness direction), filler forms dendritic aggregation in an embodiment, and it evenly is orientated at thickness direction, in Comparative Examples, observe the filler aggregation of many bulks, it is uneven and non-oriented.The SEM photo of (* y direction) is determined from composite material sheet along the Ib-Ib direction, form filler distribution state intensive and non-dense set in the composite material sheet in an embodiment, and filler forms the dendroid aggregation in intensive part.Imagine the expression that being distributed with of this filler helps high dielectric property.
Table 5
(3) pyroconductivity
Measure the pyroconductivity of the composite material sheet that is obtained in embodiment 6 and the Comparative Examples 6 according to ASTM E1530.The result is, the pyroconductivity of the composite material sheet among the embodiment 6 is 2.5W/mk, and the pyroconductivity of the composite material sheet in the Comparative Examples 6 is 1.8W/mk.Determine that from this result the composite material sheet among the embodiment has excellent pyroconductivity.Pyroconductivity is to use thermal constant measurement mechanism (Inc. makes for model TC-7000, ULVAC-RIKO) to record according to the laser flash measuring method.
(4) specific insulation
Measure the specific insulation of the composite material sheet in embodiment 7 and the Comparative Examples 7 according to JIS K7194.The result is that the specific insulation of the composite material sheet among the embodiment 7 is 5.7 * 10
12Ω cm, the specific insulation of the composite material sheet in the Comparative Examples 7 are 8.3 * 10
12Ω cm.Determine that from this result the composite material sheet among the embodiment has excellent conductivity.By using fine-adjusting current table (model TR-8641, Takeda Riken Kogyo K.K. manufacturing), DC power supply (model PLE-650-0.1, MatsusadaPrecision inc. makes) and voltmeter (model R6452A, ADVANTEST CORPORATION makes) measurement volumes resistivity.
The application is based on the patent application 2006-163909 that submits in Japan, and its content is all quoted as a reference at this.
Claims (17)
1. composite material sheet that comprises filler and organic resin matrix, wherein filler is converged into dendroid and is orientated on the thickness direction of organic resin matrix.
2. the composite material sheet of claim 1, wherein the degree of orientation of filler is greater than 1.05.
3. claim 1 or 2 composite material sheet, wherein the dielectric constant of filler is greater than the dielectric constant of organic resin.
4. any one composite material sheet of claim 1 to 3, wherein filler is at least a in inorganic particulate and the inorfil.
5. any one composite material sheet of claim 1 to 4, wherein the content with respect to the organic resin filler is 5-60vol%.
6. dielectric sheet material, it comprises any one composite material sheet of claim 1 to 5 and at least a as in the dielectric inorganic particle of filler and the dielectric inorganic fiber.
7. heat exchange sheet material, it comprises any one composite material sheet of claim 1 to 5 and at least a as in the heat conduction inorganic particulate of filler and the heat conduction inorfil.
8. anisotropic conductive sheet material, it comprises any one composite material sheet of claim 1 to 5 and at least a as in the conduction inorganic particulate of filler and the conduction inorfil.
9. method for preparing composite material sheet, wherein filler is orientated on the assigned direction of organic resin matrix, this method comprises: the step of kneading, this step comprises that with an organic solvent do not knead organic resin and filler obtain composite, this composite has the water content that is no more than 0.30wt%, and wherein filler is dispersed in the organic resin matrix; Electric field treatment step, this step comprise on the composite paint electrode, perhaps composite injected or be placed between the electrode, and apply alternating voltage, thereby filler is orientated on given direction; And fixing step, be fixed in the organic resin matrix with filler orientation.
10. method for preparing composite material sheet, wherein filler is orientated on the assigned direction of organic resin matrix, this method comprises: the step of kneading, this step comprises that with an organic solvent do not knead organic resin and filler obtain composite, this composite has the water content that is no more than 0.30wt%, and wherein filler is dispersed in the organic resin matrix; Electric field treatment step, this step comprise with resin film and are coated with composite, apply alternating voltage, thereby filler is orientated on given direction; And fixing step, be fixed in the organic resin matrix with filler orientation.
11. the preparation method of claim 9 or 10, wherein in the electric field treatment step, filler is orientated on thickness direction as the dendroid aggregation.
12. the preparation method that claim 9 to 11 is any, wherein filler has the dielectric constant higher than organic resin.
13. the preparation method that claim 9 to 12 is any, wherein filler is at least a in inorganic particulate and the inorfil.
14. the preparation method that claim 9 to 13 is any, wherein, in the step of kneading, use filler and organic resin to prepare composite, make the ratio (A/B) of dielectric constant (B) of the dielectric constant (A) of filler and organic resin be not less than 10, the particle mean size of this filler is not less than 1 μ m, and in the electric field treatment step, the alternating voltage that electric-field intensity is not less than 0.1kV/mm is applied on the composite.
15. the preparation method that claim 9 to 13 is any, wherein, in the step of kneading, use filler and organic resin to prepare composite, make the ratio (A/B) of dielectric constant (B) of the dielectric constant (A) of filler and organic resin less than 10, the particle mean size of this filler is not less than 1 μ m, and in the electric field treatment step, the alternating voltage that electric-field intensity is not less than 1kV/mm is applied on the composite.
16. the preparation method that claim 9 to 13 is any, wherein, in the step of kneading, use filler and organic resin to prepare composite, make the ratio (A/B) of dielectric constant (B) of the dielectric constant (A) of filler and organic resin be not less than 10, the particle mean size of this filler is less than 1 μ m, and in the electric field treatment step, the alternating voltage that electric-field intensity is not less than 1kV/mm is applied on the composite.
17. the preparation method that claim 9 to 13 is any, wherein, in the step of kneading, use filler and organic resin to prepare composite, make the ratio (A/B) of dielectric constant (B) of the dielectric constant (A) of filler and organic resin be set to less than 10, the particle mean size of this filler is less than 1 μ m, and in the electric field treatment step, the alternating voltage that electric-field intensity is not less than 10kV/mm is applied on the composite.
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| JP2006163909 | 2006-06-13 | ||
| JP2006163909A JP5129935B2 (en) | 2006-06-13 | 2006-06-13 | Sheet-like composite material and manufacturing method thereof |
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| US (1) | US20080102266A1 (en) |
| EP (1) | EP1867464A1 (en) |
| JP (1) | JP5129935B2 (en) |
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| JP2004193411A (en) * | 2002-12-12 | 2004-07-08 | Fujikura Ltd | Method for manufacturing high dielectric constant electric/electronic component and component |
| US7592045B2 (en) * | 2004-06-15 | 2009-09-22 | Siemens Energy, Inc. | Seeding of HTC fillers to form dendritic structures |
-
2006
- 2006-06-13 JP JP2006163909A patent/JP5129935B2/en not_active Expired - Fee Related
-
2007
- 2007-06-06 TW TW96120267A patent/TW200808544A/en unknown
- 2007-06-06 US US11/808,084 patent/US20080102266A1/en not_active Abandoned
- 2007-06-11 EP EP20070252356 patent/EP1867464A1/en not_active Withdrawn
- 2007-06-12 KR KR1020070057490A patent/KR20070118976A/en not_active Application Discontinuation
- 2007-06-13 CN CNA2007101379706A patent/CN101323173A/en active Pending
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| US9437347B2 (en) | 2009-06-22 | 2016-09-06 | Condalign As | Method for manufacturing an electrostatic discharge device |
| CN102483970A (en) * | 2009-06-22 | 2012-05-30 | 孔达利恩股份有限公司 | Electrostatic Discharge Device And Method For Manufacturing The Same |
| CN102870178B (en) * | 2010-03-17 | 2016-09-14 | 英国国防部 | To dielectric improvement |
| CN102870178A (en) * | 2010-03-17 | 2013-01-09 | 英国国防部 | Improvements in dielectrics |
| CN103190209B (en) * | 2010-10-26 | 2016-05-18 | 汉高知识产权控股有限责任公司 | For the composite membrane of plate level EMI shielding |
| CN103190209A (en) * | 2010-10-26 | 2013-07-03 | 汉高公司 | Composite film for board level EMI shielding |
| CN103384743B (en) * | 2010-12-15 | 2016-06-29 | 康达利恩股份公司 | The method forming anisotropic conductive paper and the paper being consequently formed |
| CN103384743A (en) * | 2010-12-15 | 2013-11-06 | 康达利恩股份公司 | Method for forming an anisotropic conductive paper and a paper thus formed |
| CN102779797A (en) * | 2011-05-13 | 2012-11-14 | 日东电工株式会社 | Thermal conductive sheet, insulating sheet, and heat dissipating member |
| CN102779798A (en) * | 2011-05-13 | 2012-11-14 | 日东电工株式会社 | Thermal conductive sheet, insulating sheet, and heat dissipating member |
| CN105037764A (en) * | 2015-08-03 | 2015-11-11 | 铜陵市胜达电子科技有限责任公司 | Polyimide high-dielectric composite film mixed with nano-titanium dioxide-loaded tin antimony oxide and used for capacitor and preparation method thereof |
| WO2017070898A1 (en) * | 2015-10-29 | 2017-05-04 | Boe Technology Group Co., Ltd. | Anisotropic conductive film (acf), bonding structure, and display panel, and their fabrication methods |
| CN114829505A (en) * | 2020-01-30 | 2022-07-29 | 株式会社大赛璐 | Molded body, precursor thereof, production method and use |
| CN114829505B (en) * | 2020-01-30 | 2024-05-03 | 株式会社大赛璐 | Molded body, precursor thereof, method for producing same, and use thereof |
| CN115716993A (en) * | 2022-09-30 | 2023-02-28 | 湖南大学 | Oriented high-thermal-conductivity wave-absorbing plate and preparation method thereof |
| CN115716993B (en) * | 2022-09-30 | 2024-03-01 | 湖南大学 | Oriented high-heat-conductivity wave absorbing plate and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2007332224A (en) | 2007-12-27 |
| US20080102266A1 (en) | 2008-05-01 |
| EP1867464A1 (en) | 2007-12-19 |
| JP5129935B2 (en) | 2013-01-30 |
| KR20070118976A (en) | 2007-12-18 |
| TW200808544A (en) | 2008-02-16 |
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